Refined phosphatides and process of making same



UNITED STATES PATENT OFFICE REFINED PHOSPHATIDES AND PROCESS OF MAKING SAME Philip A. Singer and Harold J. Deobaid, Peoria,

111., assignors to Allied Mills, Inc., Chicago, Ill., 7 a corporation of Indiana No Drawing. Application July 27, 1944, Serial No. 546,908

8 Claims.

phatide pastes may be omitted for this product. Due to the low oil content of the material, it is very readily dispersible in water. It is, however, easily soluble in oil and may therefore be employed in either medium.

The processes of this invention are applicable to the preparation of refined phosphatides from all types of phosphatidic residues which are commonly referred to as foots, such as may be separated from vegetable oils either by settling or by the treatment of such oils with steam, or with water, followed by centrifuging. Several types of raw materials are particularly adapted for use in accordance with the process of this invention.

phatides containing water, these products rang- One is the slimy residue which settles from crude ing from a free-flowing viscous fluid to a heavy, vegetable oils on long standing. These settlings gel-like semi-solid. or foots from hydraulic or expeller-expressed The present application is a continuation-incrude vegetable oils, such as soy bean oils, vary part of our previously filed application Serial No. in consistency from a rather hard, waxy lower 494,116, filed July 9, 1943, now abandoned. layer to a thick, slimy, oil-like upper layer. In

Commercial phosphatides, now available usually in the form of heavy oily liquids or thick oily pastes, have a relatively high oil content. These products present considerable difiiculties in handling and transportation due to their physical natures. In addition, this high oil content inhibits their direct dispersibility in water. An oil carrier in many instances is detrimental to processes in which the phosphatide may be used. Any oil present also acts as a diluent, reducing the actual content of phosphatide in the final lecithin product.

Methods for the production of dry or pulverulent forms of phosphatides have previously been suggested. In manufacturing these products, however, there are involved the use of organic solvents or chemical treatment, or both, for the purification of the material. Some oil-absorbing material is also usually employed to take up the excess oil in order to obtain the desired stable pulverulent form. By prior processes, refined phosphatides or phosphatides having a low oil content tended to become rancid within a few weeks. In contrast therewith, our product, as herein described, has proven stable and would remain fresh for extended periods under a broad range of storage conditions.

The present invention yields, aside from others, a product which is unique and novel in that it has an unusually high phosphatide content, containing only some 15 per cent oil, containing no added extraneous materials, and one which in its final finished form is a solid light-colored flake. Since its color is light, the operation of bleaching as now ordinarily applied to commercial phosgeneral it is preferred to use the lower layer of such oil settlings or foots, since it has been found to have a higher phosphatide content. However, the upper slimy-like layer may be used to advantage by separating the surplus oil therefrom in a centrifuge. Another source of foots, which are of slightly different character, is the residue obtained from a crude expressed vegetable oil which has been washed with water or steamed. The foots from oils so treated may be separated from the oil by centrifuging. Still another source of foots, which may be of slightly different character, is the residue obtained from steam or watertreated solvent-extracted oils. It will be recognized, however, that in accordance with this invention, phosphatidic residue from vegetable oils obtained by any process may be used. In the following description and in the appended claims, the crude phosphatidic raw material which may be treated in accordance with this invention will be termed foots, and this term as used herein is intended to cover any phosphatidic raw material indicated briefiy in the foregoing, or commonly designated as such in the trade.

The use of organic solvents, such as acetone, hydrocarbons, chlorinated hydrocarbons, esters, alcohols, etc., has generally characterized most previous processes for obtaining refined vegetable phosphatides from the crude products obtained by water-washing vegetable oils or from tank settlings of stored crude vegetable oil. The use of such solvents involves not only extra expense for material and equipment, but also may introduce serious fire, explosion, or health hazards in industrial operations. In accordance with the presa refined phosphatide may be produced from oil foots by first emulsifying the ioots with a quantity of water, thereafter causing the emulsion to break and mechanically separating a refined phosphatide from the thus broken emulsion. The

vegetable oil foots that maybe used in accordance with the processes of this invention may be any of those indicated in the foregoing and are preferably obtained from soy bean oil which contains substantial quantities of phosphatides, princilpally cephalin and lecithin. Other phosphatide-' containing oil foots may be obtained from corn oil, cottonseed oil, peanut oil, etc.

Incarryi'ng out the process of this invention.

particular attention should be given to the temperature ,and concentration relationships both in emulsifying and in breaking the emulsions so that the process may be easil carried out, and so that an improved product will be formed. In accordance with one embodiment of this invention, a vegetable oil foots containing a substantialquantity of vegetable phosphatide is emulsified with a definite quantity of water and thereafter heated in order to produce a mass having a stiff, dough-like consistency. Thereafter the dough-like mass is cooled, allowed to stand until it has separated ,into three distinct layers, namely, an upper oil-containing layer, an intermediate .water-containing layer, and a lower phosphatideecontaining layer. This lower phosphatide-containing layer, may then be separated from the remaining layers as the desired product of the process. In this particular process it is important that the amount of water used for emulsifying the phosphatidic residue be closely regulated so that a dough-like mass is produced which will separate in the manner indicated in the foregoing. A mass having the proper consistency will be eificiently formed when the water in the emulsion falls within the range of between about 4.5 and 5.5 times the weight of the phosphatide initially present in the foots to be treated. The amount of phosphatide present in the roots may be ascertained by chemical analysis as a guide to the proper amount of water to be employed.

, In accordance with a further embodiment of this invention, the oil foots may be emulsified with water, and the phosphatide-containing material may be coagulated or precipitated by the addition of a water-soluble electrolyte to the emulsion. The water-soluble electrolyte may be sodium chloride, potassium chloride, acetic acid, hydrochloric acid, sulfuric acid, phosphoric acid, or the like. However, a noncontaminating divalent metallic salt, such as calcium chloride-or trivalent metallic salt, such as aluminum chloride or aluminum sulfate, is preferred for this step of the process. When the phosphatidic sol or gel is coagulated or precipitated with an electrolyte, the amount of water present in the phosphatide emulsion may fall considerably outside of the range indicated above for the process when Water alone is used to purify r refine the phosphatide present in the foots.

One object of the present invention is the provision of a process for producing a refined vegetable p hat dasuc a es iai 1yesB- table oil phosphatidic residues without neces- 'sitating the use of organic solvents, without precise control of acidities, and without cautious additions of electrolyte as required by previously employed processes.

An additional object oi the present invention is to provide a vegetable phosphatide which is exremely active for reducing the viscosity of plastic chocolate compositions.

A further object of the present invention is the provision of a water-containing phosphatide gel preparation which may be used directly for reducing the viscosity of such materials as plastic chocolate compositions or which may be dried and mixed with any selected oil for the same purpose.

A further and additional object of the prose it invention is the provision of a refined phosphatide gel composition containing substantial quantities of water, but which may be admixed with a previously dried phosphatide preparation to produce a product having any desired moisture content. 7

A further and additional object of the present invention is the provision of a process for preparing a light-colored vegetable phosphatide product from vegetable oil roots. 7

A further and additional object of the present invention is the preparation of a light-colored lecithin product in flake form, high in phosphatide content, and having marked emulsifying and thinning properties as well as high antioxidant activity. 4

Further and a'dditional objects will appear from the following description and the accompanying claims. 7 p r For a more complete understanding of the present invention, reference will now be had to the following examplesvl herein several specific processes are disclosed showing how this invention may be used. Itwill be understood, however, that these designated processes are given only by way of examp e and it is not intended that the invention be in any way limited thereto.

Example 1 One hundred pounds of soy expeller oil roots containing approximately eilper cent of phosphatides are first emulsifiedwith 192 pounds of water. Emulsiiication be hastened by vigorous agitatio and sometimes assisted by warming. In this particular example, the amount of water used for emulsifying he ioots is about 4.8 times the weight of thephosphatide contained inthe foots asdetermined by chemical analysis. After emuisifying, the mixture is heated in a steam jacketed tanl; or by other suitable means to the boiling point. H parently series of complex physical (and possibly chemical) changes occur durin theheating process, resulting, at or soonafterthe boiling point has been reached, in theemulsion becoming a thick homogeneous mass having peculiar dou hy properties. This doughy productis allowed to boil or is maintained at near boiling temperatures for 30 to 35 minutes with mild agitation and with the addition of water to replace that ay have been lost by evaporation. H h emulsion has been found to maintain during 7 iis period the physical characteristics of a dough. The time of heating this dough-likernass does not appear to be critical, andeicperiments have shown that heating may vary from 5 or 10 minutes to over one hour vvithsatisfactory results. v

3 ...i?h? iqm q s m ss .bii boiled as described above, it is allowed to cool. During the initial cooling stage, slight stirring may prove advantageous, but agitation should not be continued after the first few minutes or after the mix has been cooled to about 80 C. After allowing the dough to cool to about 50 0., the mix is held at this temperature until the doughy emulsion slowly breaks, that is, separates into three distinct layers. This separation will usually be completed after four to 48 hours. Although in this process doughs may vary somewhat in such respects as appearance, rate of separation, and composition, depending upon their source and manner of emulsification, it is the unique property of separating cleanly into these three phases or layers which characterizes the proper type of dough produced as described, by proper dilution and temperature control in the process.

Under various conditions the volume of the top layer finally separating may vary from 5 to 25 .per cent of the total mass, depending on the purity of the raw material, the amount of water employed, and the amount of oil in the original f-oots, i. e., in the type of foots involved. This top layer contains oils, gums, and other impurities. It also may contain very small amounts of phosphatides. The middle or intermediate layer may amount to about 5 to 25 per cent of the total mass and is usually a clear watery solution containing very small amounts of phosphatides and some soluble carbohydrates. The third or lowest layer usually amounts to about 50 to 75 per cent of the total mass and may contain 85 per cent or more of the total phosphatides of the raw material. This lower layer may also contain oil, usually to the extent of not more than one-fourth of the amount of phosphatide present, and varying amounts of water. This lower layer is known as the phosphatide gel layer, or sometimes as the phosphatide layer.

If in the above indicated process an emulsion is prepared using too little water, or if water, evaporated during emulsification and subsequent heating, is not replenished, two disadvantageous effects will be encountered. First, the proper separation of the doughy emulsion, which appears to depend on the collodial condition or state of dispersion to produce ultimately a clean rapid separation of the oil from the hydrated phosphatide, will not properly occur and the line of separation between the top 011 layer and the bottom hydrated phosphatide layer will be indistinct if the intermediate water layer is lacking. Consequently, separations of oils from phosphatides under these conditions are incomplete and difi'icult. Accordingly, when the emulsion is heated as above described, additions of water should be made from time to time so as approximately to maintain the original water-phosphatide ratio of the emulsion as stated above. The production of the proper dough phase is an important step in this modification of this process wherein only water is used as a separating agent. The production of the dough under centain controlled conditions, or what may be termed the change from a free-flowing liquid mass to a doughy or plastic mass. This point is readily detectable and is easily reproducible. If the amount of water present is now determined, it will be found to be quite close to a ratio of 5.4 of water to 1 of phosphatide, which is a convenient ratio for practical purposes. For optimum phosphatide recovery, the optimum water ratios are from between 4.7 to 5.0 parts of water to one part of phosphatide for foots containing 35 to 45 per cent phosphatides. These ratios furnish the amount of water which will produce a suitable emulsion resulting in an efficient and facile separation within a reasonable time into the several component layers, the bottom layer of which is a refined hydrated phosphatide. For foots of higher or lower phosphatide content corresponding variations from these ratios may be advisable. However, the water ratios may be varied between about 4.5 and 5.5 or slightly higher, in which latter case decreased efiiciency will be encountered. Below 4.5 the dough is usually too stiif to permit of clean separation of the components into layers. When the ratio is much above 5.5, it ordinarily takes too long to obtain the separation, the separation is quite often incomplete, and the resulting product contains excessive quantities of oil. However, in some cases, because of such practical considerations as ease or speed of working, slightly higher water ratios than the optimums 4.7 to 5.0 suggested may prove preferable despite their lower yields. Where the water ratio is increased to 5.5, the recovery of phosphatide from soy expeller oil foots will be found to decrease by one to 4 per cent, depending upon the exact nature of the foots.

The foregoing example typifies optimum conditions for the separation of phosphatides from soy expeller foots containing usually 30 to 50 per cent phosphatide, 40 to 50 per cent oil, some carbohydrate, and some free fatty acid, sterols, fiber, grit, etc.

The following examples set forth other procedures that may also be useful under certain conditions.

Example 2 One hundred pounds of soy expeller oil foots containing 40 per cent crude phosphatide are emulsified by strong agitation with 600 pounds of water. In this modification of the process the ratio of water to phosphatides of about 15 to 1 was found to produce the most satisfactory isolation of phosphatides from other constituents of the foots, particularly from water-soluble carbohydrates. The resulting emulsion is then heated to about 77 C. with stirring and maintained at this temperature for 30 minutes with continued stirred. One and one-half pounds of calcium chloride in a 20 per cent water solution are then added to the mixture with continued stirring, and the temperature is gradually increased to about 82 C. The calcium chloride electrolyte breaks the emulsion, the crude lecithin or vegetable phosphatide precipitating out in a doughy mass from which most of the water is easily poured away after kneading the mass while ,still warm. In this step most of the soluble carbohydrates are dissolved out. It will be noted that in this example, when an electrolyte is used for precipitating or coagulating the vegetable phosphatide, much higher water ratios in the emulsion are found to be desirable. I

The dough precipitate is then made up al- :most tothe original volume bythe additionpffiOO pounds or Water and ism-emulsified by irring at about 509.6. The emulsion formed is then heated to about 75 .to 80 .C. and .is thereafter allowed .to cool slowly to about 2 :0. wi h agitation. It is then allowed tostand for 2,4 to

48 hours at about 20 -,C. This mass then separates into three layers as described in connection with Example 1. The lowermost layer here is the desired purified .phosph tide eel. Sufficientcalcium chloride remains in the first precipitate again to induce coagulation at the elevat d t mperatures where y s paration at the lower temperature is made possible. However, the second ,emulsification and re-precipitation reduces .the calcium chloride concentration belowzthe taste threshold and the traces of calcium chloride present .in the final pr duct have :sub-

stantially no efiect on the emulsifying power'of the phosphatide prepared by this method.

Example 3 This is a modification of the process of Example 2 supra. One hundred pounds of foots are emulsified .by strong agitation with 600 pounds of water at .30" C. This mixture is heated to about 77 C. and held at that temperature with mild agitation for about one-half hour. This emulsion .is then treated with two pounds of calcium chloride dissolved in water, and .forms a precipitate or coagulum as described in the preceding example. This coagulum .is re-emulsified in the same solution by stirring and cooling rapidly to 20 C. The resulting doughy imass is then allowed to stand without agitation for 24 to 48 hours, during which time it separates into the three layers previously described. The lower layer is then separated from the others and is the refined phosphatlde gel prepared in accordance with one modification of this invention.

Example 4 In accordance with one embodiment of this invention, the emulsion of foots and water in the absence of a coagulating-electrolyte maybe heated to above the atmospheric boiling point. In accordance with this example, 106 pounds of facts are emulsified with 250 pounds of water and then heated to about '60" C. and allowed to remain at this temperature with mild agitation for about 60 minutes. The resulting emulsion is then heated under about 25 pounds pressure to about 139 C. with agitation, the heat being so adjusted as to bring about this rise in-temperature in about 20 minutes. The pressure ismaintained for about five minutes and the resulting doughy mass is allowed to cool in ya quiescent state to about 58 C. and to remain at this temperature for about 24 hours. This mass separates :into three layers as described above.

In this example the water phosphatide ratio is somewhat greater than that specified as being desirable in Example 1. However, this is due to the fact that a certain amount of water is required to provide Water vapor to bring the pres- I Example 5 As another variationof the process of this inyention it has been found possible to apply electro-phoresis .or electroesedimentation in accelerating the precipitation of .the. lower phosphatide layer from suspension as demonstrated in the following procedure: Ten pounds of foots were emulsified by strong agitation with 30 pounds of water and immediately subjected to 100 volts potential. A gel .separation occurred within one hour. In common with other electro-phoretic or electro-sedimentation processes, the process of .this example depends upon many conditions which may be .diflicult to control, such as the state of dispersion of the phosphatides and the conductivity .of the emulsion.

The preceding examples are merely illustrative and should not be considered as in anyway restricting the process of this invention. It will become apparent from experiments that time, temperature, water-'foots ratio, and perhaps acids or inorganic salt concentration (when used in the process) are determining factors in establishing the proper condition for the formationof the gel or sol which separates in the manner indicated above. It is obvious that results of, a kind may be attained for any foots-waterratio through treatmentwith electrolytic and proper processing. Electrolytes do not form an essential partof the process. Also it is obvious that for any given temperature of operation a suitable Water concentration and treatment may be developed in order to obtain results.

In the three layers which separate .from the water emulsion of foots as described in the foreug, the lower layer has been found to be .a heavy, gel-like, brown liquid which may beseparated easily by any convenient means from the top layers. This may preferably bedoneasabove described by gravity separation. However, cen trituging may also be employed if desired. This product, when dried at lil0 C..--in ,air or at a lower temperature in mono, yields a product containing approximately v8i .per .cent'phosphatide.

Oil susceptible to further refinement may be recovered from the top :layer and constitutes a valuable by-product of the process of this invention. Another iuseful by-tproduct is the water layer which has been foundto contain-substances having anti-oxidant properties.

We have found :that the phosphatide gel described in each of the above examples may be dried to produce a novel form ofphosphatide having unique chemical and physical properties. The dried material, a product :of this invention, is readily dispersible in water, soluble in oil, and hasvery marked emulsifying and thinning prop- .er-ties, through its effects on surface tension modifies the colloidal nature of suspensionsand of foams to improve their stability. It is'a solid wax-like product in flake form, very stable at ordinar temperatures and practically non-hygroscopic. This product is, in addition a strong anti-oxidant is valuable as .a stabilizer for fats and oils, vitamin preparations brother materials subject .to deterioration by oxidation.

The phosphatide content of the material is approximately percent, and because of its ready dispersibi-lity .in'water, together with its high purity, it is especially advantageous in biscult, cracker and-confectionery formulas and in all cases where aqueous media are desirable. Its leady solubility in oil makes it applicable .in all instances where commercial phosphaticles are now used, and the oil used for the solution .of the flake may be selected for its adaptability to any product or process in-Which it is to be used. This eliminates the necessity .for using oils which may be undesirable or detrimental to any given process or product.

The primary advantage of this dry, solid, waxy, flaked product is that it is readily dispersible in water and readily soluble in oil, thus adapting it for use in either medium or in any combination or formula in which both oil and water are employed. The phosphatide may be added according to convenience or practicability directly to a formula before being mixed or during mixing, in many cases lending its thinning value to reduce the power required for mixing, as in the preparation of an ointment or pigmented oil, or .it may be added to a finished product and readily dispersed therein as in molten chocolate liquor to produce a controlled reduction in viscosity. It may be dissolved in water or other liquid component and thus be added in solution as in the preparation of emulsions, or it may be added with solid constituents as, for example, in so-called lecithinized flours used in preparing doughs. The flake may be added advantageously to cocoa beans before grinding them for the preparation of chocolate in order to reduce grinding power requirements and to increase yield.

Another advantage of this product is its physical state, a stable, solid, waxy, practically nonhygroscopic flake. The product in this form greatly facilitates handling, packaging and transportation. The flake may be poured, shoveled or otherwise more conveniently handled than the pastes. Because of its dry form the flake can be quickly, easily and completely emptied from its containers, thus efiecting savings in time and materials; pastes cannot be removed completely from their containers except by laborious scraping, and even after scraping almost invariably some paste is lost by being retained on the walls or in the corners of thecontainers. reasons weighing portions of flake becomes a simpler operation since the dry form phosphatide can be poured into and out of weighing vessels with utmost convenience and speed and allows' quantitative delivery without careful, laborious scraping. Lightweight, nonmetallic, cheap containers may be used for the flake instead of heavy, costly metallic or glass vessels as used presently for the oils and pastes. Still another advantage For similar is its low oil content which adapts the material w"- A still further advantage is the unusual em- 5 ciency of the product as an emulsifying and thinning agent.

Still another advantage is the stability of the material which enables it to be stored or trans-.

ported for long periods of time without danger of spoilage or detrimental change in the physical character of the product.

For the preparation of this product, the phosphatide gel may be introduced without further treatment onto a standard atmospheric drum drier. Such a drum drier consists of two parallel, hollow metal cylinders mounted horizontally adjacent to each other, coupled and driven to rotate toward each other when viewed from above, and internally heated with steam at a pressure of usually not more than 80 pounds, preferably -50 pounds, The space between the drums may be varied. The phosphatide gel, separated as a bottom layer in the above-described refining process for phosphatides, may be fed directly into the trough formed by the adjacent upper quadrants of the drier drums. Upon contacting the heated drums, a layer of the gel adheres to the surface of each drum and is carried through the space between the drums, the thickness of the emerging adherent layer or film being regulated by adjusting the distance between the drums. At proper rotational speed, film thickness and drying temperature, the adherent phosphatide film becomes dried in less than one revolution of the drum to a sheet which can be readily removed by a scraper. The resulting dry phosphatide sheet as it is disengaged from the rolls is warm enough to have a tensile strength sufficient to carry it from the rolls without difficulty. On cooling, the sheet becomes brittle and may be easily broken into flakes of any desired size by an agitating device such as a high speed beater which will break up the sheets without exerting any considerable friction on the material.

If desired, the bottom layer of phosphatide gel described in each of the examples cited may be further purified and partially dehydrated by treatment with calcium chloride or otherinorganic salts and acids. In accordance with one embodiment of this re-purification process, the phosphatide gel is diluted with two volumes of water and stirred and heated to about 65 to 75 C. At this point a 20 per cent calcium chloride solution is added slowly with mild stirring. Violent agitation is to be avoided, since air may be introduced into the mixture which causes the coagulum to rise to the urface, making separation difficult. The mild stirring is continued until the phosphatides have precipitated out of the solution, the amount of dry calcium chloride required being roughly 0.2 per cent by weight of the diluted gel. The phosphatides then settle to the bottom of the tank or other container and the separated liquor may be drawn off. If de* sired, the phosphatides may be separated more rapidly by centrifuging. Other electrolytes which may be substituted for the calcium chloride in this re-purification step may be inorganic salts, such as ferric chloride, and certain bleaching agents, and also acids, such as sulfuric acid. Any of the separated lower layers of partially refined phosphatides after being kneaded to remove ex.-

cess water, becomes a gel-like mass containing about per cent of water, about 10 per cent of oil or free fatty acids, and about 30 per cent of phosphatides. One important and valuable characteristic of this process is that the gel-like phosphatidic product, whatever its water content, has a substantially uniform composition with respect to its phosphatide and oil content when cal-: culated on a moisture-free basis.

Further dehydration of the phosphatidic gel may be accomplished by heating and kneading out additional quantities of water so that the re-: sulting mass after cooling contains 40 to 50 per cent moisture and is physically quite stable, The product thus obtained dissolves easily in water or in oil and has extremely high emulsifying properties and chocolate-thinning action. Attention is directed to the fact that this product, containing 40 per cent or morev of moisture, has been found to have a marked thinning effect .on molten chocolate, equal to or higher thanother commercial vegetable phosphatides, all of which 13 sodium chlorite is added to the doughy mass to bleach the phosphatide contained therein.

7. Process of recovering a refined vegetable phosphatide from vegetable oil foots containing substantial quantities of such phosphatides which comprises emulsifying said foots with an amount of water equivalent to about fifteen times the total weight of the phosphatides present in said foots, heating the resulting emulsion to about 77 C. while stirring for about 30 minutes, thereupon adding suflicient quantity of an electrolyte to break said emulsion to efiect the separation therefrom of a doughy mass, kneading the latter and then decanting separated aqueous solution of electrolyte therefrom; diluting the residual material to a volume about equal to that of the orginal emulsion and heating it to about 75 to 80 C. and then slowly cooling it to about 20 C. and allowing it, in the course of from about 24 to 43 hours to stratify into three layers; separating the lowermost layer which contains the desired phosphatide, and recovering the sion and to precipitate the phosphatide; re-emulsifying said precipitated phosphatide in the original solution by again heating and then cooling the re-formed emulsion to about 20 C. and gravity-separating it to form three layers; and separating the lowermost layer which contains the desired phosphatide, and recovering the latter.

PHILIP A. SINGER.

HAROLD J. DEOBALD.

REFERENCES CITED The following references are of record in the file of this patent:

UNITED STATES PATENTS OTHER REFERENCES Horvath The Soybean Industry, pages 113- 114, Chem. Publ. Co., N. Y., 1938. 

1. A PROCESS OF RECOVERING A REFINED PHOSPHATIDE FROM OIL FOOTS CONTAINING SUBSTANIAL QUANTITLES OF PHOSPHATIDE WHICH COMPRISES EMULSIFYING SAID FOOTS WITH WATER IN AN AMOUNT BETWEEN ABOUT 4.5 AND 5.5 TIMES THE TOTAL WEIGHT OF THE PHOSPHATIDE PRESENT IN THE FOOTS, HEATING THE RESULTING EMULSION TO A TEMPERATURE AND FOR A TIME SUFFICIENT TO PRODUCE A PRODUCT HAVING A DOUGH-LIKE CONSISTENCY, COOLING THE RESULTING MASS, GRAVITY-SEPARATING SAID MASS WHEREBY THREE LAYERS ARE FORMED, SEPARATING THE LOWERMOST LAYER FROM THE OTHERS AS THE DESIRED PRODUCT. 